CN104950060B - Based on chromatograph-spectrogrph combination and the analysis method of the paeonol content of subspace angle criterion - Google Patents
Based on chromatograph-spectrogrph combination and the analysis method of the paeonol content of subspace angle criterion Download PDFInfo
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Abstract
The invention discloses a kind of analysis method based on the combination of chromatograph spectrogrph with the paeonol content of subspace angle criterion, specifically implement according to following steps: paeonol standard spectrum storehouse is set up, the preparation of sample to be tested and ultraviolet spectra collection, the foundation of modeling Fundamental database, content detection of paeonol in sample to be tested.It is combined herein by liquid phase ultraviolet-visual spectrometer, application subspace angle criterion, establishes paeonol content rapid analysis method.For the mensuration of similar sample, and only need to once model just can batch detection.Compared with high performance liquid chromatography, the method set up is reliable and stable, easy and simple to handle, sample need not the pre-treatment of complexity, quickly measures for paeonol content and provides a kind of practical quantitative analysis tech, and can be applied to other paeonol goods detection field.
Description
Technical field
The invention belongs to pharmaceutical analysis technical field, be specifically related to a kind of based on chromatograph-spectrogrph combination and
The analysis method of the paeonol content of subspace angle criterion.
Background technology
Paeonol is extract a kind of Chinese crude drug out from the root bark of the national flower Flos Moutan of China.Extract
From the dry root bark of ranunculaceae peony.Paeonol pharmacology action is worth extensively, except for medical preparation
Outside raw material, it is additionally operable in the daily use chemicals product such as toothpaste, skin protection, beauty treatment.The assay of paeonol is various systems
One of leading indicator of agent and control of product quality.Paeonol content analysis at present uses high-efficient liquid phase color more
Spectrometry, this method sensitivity is high, but analysis cost is high, and manipulation strength is big, and the analysis efficiency of sample is low in high volume,
Need to set up a kind of quick analyzing novel methods of paeonol content.
Summary of the invention
It is an object of the invention to provide a kind of based on chromatograph-spectrogrph combination and the pellet of subspace angle criterion
Skin phenol method Han quantitative analysis, solve that analysis efficiency present in prior art is low, manipulation strength greatly with
And the problem that analysis cost is high.
The technical solution adopted in the present invention is, a kind of based on chromatograph-spectrogrph combination and subspace angle
The analysis method of the paeonol content of criterion, specifically implements according to following steps:
Step 1, paeonol standard spectrum storehouse are set up,
Step 2, the preparation of sample to be tested and ultraviolet spectra collection,
Step 3, the foundation of modeling Fundamental database,
Content detection of paeonol in step 4, sample to be tested.
The feature of the present invention also resides in,
Paeonol standard spectrum storehouse is set up particularly as follows: prepare the paeonol that series concentration is 0.2～20mg/L
Standard solution, with 75% ethanol as blank, gathers the 190nm-1100nm wave-length coverage light of serial solution
Spectrum；Select 200nm-400nm wave-length coverage spectrum, after multivariate least square regression, obtain Cortex Moutan
Phenol standard spectrum yi=aix+bi, it is designated as V, wherein linear equation and correlation coefficient at 270nm divide
It is not: y=0.0792x-0.0636；R=0.9992.
Preparation and the ultraviolet spectra collection of sample to be tested are particularly as follows: take paeonol crystalline mother solution, under room temperature,
Take 0.15g upper solution and each portion of underlying crystalline respectively, with 75% ethanol dilution to concentration be
10-20mg/L, obtains sample S1And S2；
Take the paeonol crystalline mother solution two parts of different production batch, be separately heated to 50 DEG C and become molten condition,
Weigh 1.2g and 0.9g respectively, be 10-20mg/L with 75% ethanol dilution to concentration, obtain sample S3
And S4；
Weigh paeonol crystalline product 0.1g, be 10-20mg/L with 75% ethanol dilution to concentration, obtain
Sample S5；Take S1-S5Equal-volume is mixed to get sample S6；
Gather S1-S6Ultraviolet spectrum data, obtain sample to be tested data base, be designated as D；The time of integration
15 microseconds, integral number of times 20 times, wavelength 200-400nm.
Step 3 models the foundation of Fundamental database particularly as follows: to testing sample S1-S6Compare with paeonol
Product sample B3, be combined by liquid chromatograph and spectrogrph, gather various kinds this after chromatographic column is kept completely separate
Multi-wavelength light modal data；The spectrum number of component paeonol to be measured is deducted from testing sample spectroscopic data
According to, and through Data Dimensionality Reduction, obtain background spectra database N；
Liquid phase chromatogram condition: 4.6mm × 150mm C18Post；Gradient elution, flow phase: 0～30min,
Acetonitrile: water=40:60 (V/V)；30～55min, acetonitrile: water=5:95 (V/V)；55～80min,
Acetonitrile: water=95:5 (V/V)；Flow velocity 1mL/min；Sample size 20 μ L；Column temperature 20 DEG C；Chromatograph is examined
Survey wavelength 270nm；Spectral conditions: floating cuvette 1cm；The time of integration: 15 microseconds；Integral number of times:
20 times；Ultraviolet detection wavelength: 200-400nm.
In the dimensionality reduction of background spectra database, described background spectra database W is reduced to suitable dimension
Method as follows: application [U, S, V]=svd (W) carries out singular value to background spectra database W and divides
Solve dimensionality reduction, after decomposition, obtain matrix with orthogonal rows U, n rank, m rank row orthogonal matrix V and singular value matrix S,
Take the front q row of U, for the Fundamental database N after dimensionality reduction.
Content detection of paeonol in sample to be tested is particularly as follows: by above-mentioned standard spectral data storehouse V, bias light
Modal data storehouse N and D imports and calculates platform, chooses 200-400nm wavelength period, and application vector-son is empty
Between angle criterion algorithm calculate the content of paeonol in each sample to be tested respectively.
The concretely comprising the following steps of content detection of paeonol in sample to be tested:
Step 4.1, foundation quantitative accuracy set and reduce step delta；
Step 4.2, at formula yi=aix+biIn bring bigger x into1Value, obtains v1；
Described yiRepresent the absorbance of paeonol, a under i wavelengthi、biBeing constant, x represents hydroxyl
The concentration of yl benzoic acid, v1Represent in concentration to be x1Time paeonol multi-wavelength absorbance y1, v1For institute
Some yiThe matrix of value composition；
Step 4.3, from sample to be tested spectroscopic data a deduct v1/ Δ, the variable after deduction is designated as da；
Background spectra database N and variable da are merged postscript for contrast space M, calculate contrast space M with
v1Angle；
Step 4.4, from sample to be tested spectroscopic data a, progressively deduct v1After, repeat step (3)；
Step 4.5, after the paeonol in sample to be tested is deducted completely, comparison space M and paeonol
Spectral vector v1Space angle value there will be maximum θmax, record space angle maximum θmax
Corresponding during appearance reduce step number λ, by concentration x of paeonol1Estimate in sample to be tested with reducing step number
The content Y of paeonol1, calculating formula is Y1=X1× λ/Δ, the Y obtained1It is Cortex Moutan in sample to be tested
The content value of phenol.
The invention has the beneficial effects as follows: first build paeonol standard database, then by not
Carry out a high performance liquid chromatography-spectrogrph combination with batch paeonol crystalline mother solution sample, gather various kinds
Product spectroscopic data after chromatographic isolation, processes through data and obtains this truth of a matter without tested component paeonol
According to, paeonol content in direct analysis sample to be tested can be realized in conjunction with space angle criterion algorithm.Lead to herein
Cross liquid phase-ultraviolet-visual spectrometer combination, apply subspace-angle criterion, establish paeonol content fast
Speed analysis method.For the mensuration of similar sample, and only need to once model just can batch detection.With height
Effect liquid phase chromatogram method is compared, and the method set up is reliable and stable, easy and simple to handle, and sample need not complexity
Pre-treatment, quickly measures for paeonol content and provides a kind of practical quantitative analysis tech, and can
It is applied to other paeonol goods detection field.
Accompanying drawing explanation
Fig. 1 is paeonol mother solution and the liquid chromatogram of paeonol reference substance.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
The present invention provides a kind of based on chromatograph-spectrogrph combination and the paeonol content of subspace angle criterion
Analysis method, specifically according to following steps implement:
Step 1, paeonol standard spectrum storehouse are set up,
Preparation series concentration is the paeonol standard solution of 0.2～20mg/L, with 75% ethanol as blank,
Gather the 190nm-1100nm wave-length coverage spectrum of serial solution；Select 200nm-400nm wave-length coverage
Spectrum, obtains paeonol standard spectrum y after multivariate least square regressioni=aix+bi, it is designated as V,
Wherein linear equation and correlation coefficient at 270nm are respectively as follows: y=0.0792x-0.0636；R=0.9992.
Step 2, the preparation of sample to be tested and ultraviolet spectra collection,
Take paeonol crystalline mother solution, under room temperature, take about 0.15g upper solution respectively and underlying crystalline is each
Portion, is 10-20mg/L with 75% ethanol dilution to concentration, obtains sample S1And S2。
Take the paeonol crystalline mother solution two parts of different production batch, be separately heated to 50 DEG C and become molten condition,
Weigh 1.2g and 0.9g respectively, with 75% ethanol dilution to 10-20mg/L, obtain sample S3And S4。
Weigh paeonol crystalline product 0.1g, with 75% ethanol dilution to 10-20mg/L, obtain sample S5；
Take S1-S5Equal-volume is mixed to get sample S6。
Gather S1-S6Ultraviolet spectrum data, obtain sample to be tested data base, be designated as D.The time of integration
15 microseconds；Integral number of times 20 times；Wavelength 200-400nm.
Step 3, the foundation of modeling Fundamental database,
To testing sample S1-S6With paeonol reference substance sample B3, it is combined with spectrogrph by liquid chromatograph,
Gather this multi-wavelength light modal data after chromatographic column is kept completely separate of various kinds, from testing sample spectroscopic data
The spectroscopic data of middle deduction component to be measured paeonol, and through Data Dimensionality Reduction, obtain background spectra database N.
Liquid phase chromatogram condition: C18Post (4.6mm × 150mm)；Gradient elution, flow phase: 0～30min,
Acetonitrile: water=40:60 (V/V)；30～55min, acetonitrile: water=5:95 (V/V)；55～80min,
Acetonitrile: water=95:5 (V/V).Flow velocity 1mL/min；Sample size 20 μ L；Column temperature 20 DEG C；Chromatograph is examined
Survey wavelength 270nm.
Spectral conditions: floating cuvette (1cm)；The time of integration: 15 microseconds；Integral number of times: 20 times；
Ultraviolet detection wavelength: 200-400nm.
Content detection of paeonol in step 4, sample to be tested.
Above-mentioned standard spectral data storehouse V, background spectra database N and D are imported Matlab calculate
Platform, chooses 200-400nm wavelength period, and application vector-subspace angle criterion algorithm (is called for short VS
Method) calculate the content of paeonol in each sample to be tested respectively；
Wherein, in sample to be tested content detection of paeonol particularly as follows:
Step 4.1, foundation quantitative accuracy set and reduce step delta；
Step 4.2, at formula yi=aix+biIn bring bigger x into1Value, obtains v1；
Described yiRepresent the absorbance of paeonol, a under i wavelengthi、biBeing constant, x represents Cortex Moutan
The concentration of phenol, v1Represent in concentration to be x1Time paeonol multi-wavelength absorbance y1, v1For all of
yiThe matrix of value composition；
Step 4.3, from sample to be tested spectroscopic data a deduct v1/ Δ, the variable after deduction is designated as da；
Background spectra database N and variable da are merged postscript for contrast space M, calculate contrast space M with
v1Angle；
Step 4.4, from sample to be tested spectroscopic data a, progressively deduct v1After, repeat step 4.3；
Step 4.5, after the paeonol in sample to be tested is deducted completely, comparison space M and paeonol
Spectral vector v1Space angle value there will be maximum θmax, record space angle maximum θmax
Corresponding during appearance reduce step number λ, by concentration x of paeonol1Estimate in sample to be tested with reducing step number
The content Y of paeonol1, calculating formula is Y1=X1× λ/Δ, the Y obtained1It is Cortex Moutan in sample to be tested
The content value of phenol.
Embodiment 1
1 experimental section
1.1 instruments and reagent
High performance liquid chromatograph (LC-20AT, Shimadzu)；Ultraviolet-visible fiber spectrometer (Maya2000,
Ocean Optics)；Electronic analytical balance (AL104, prunus mume (sieb.) sieb.et zucc. Teller-torr benefit)；Ultrasonic washing unit
(the letter Instrument Ltd. in Shanghai)；Dehydrated alcohol (AR), methanol (chromatographically pure), acetonitrile (chromatograph
Pure), paeonol reference substance (purity 99.9%), (Guangxi hundred million health pharmacy industry is limited for paeonol crystalline mother solution
Company).
1.2 test method
1.2.1 paeonol standard spectrum storehouse is set up
Accurately weigh 0.1010g paeonol reference substance, with 75% ethanol constant volume to 100mL.Prepare successively
Concentration is 2mg/L, 4mg/L, 8mg/L, 12mg/L, 16mg/L, 20mg/L paeonol-75% ethanol
Solution B1-B6.Gather each solution 200nm-400nm ultraviolet spectra, obtain standard through least square regression
Library of spectra V.
1.2.2 the preparation of sample to be tested and ultraviolet spectra collection
Take the paeonol crystalline mother solution that manufacturing enterprise provides, under room temperature, take about 0.15g upper strata respectively molten
Liquid and each portion of underlying crystalline, with 75% ethanol dilution to finite concentration, obtain sample S1And S2。
Take the paeonol crystalline mother solution two parts of different production batch, be separately heated to 50 DEG C and become molten condition,
Weigh 1.2g and 0.9g respectively, with 75% ethanol dilution to finite concentration, obtain sample S3And S4。
Weigh paeonol crystalline product 0.1g, with 75% ethanol dilution to finite concentration, obtain sample S5。
Take S1-S5Equal-volume is mixed to get sample S6。
Gather S1-S6Ultraviolet spectrum data, obtain sample to be tested data base, be designated as D.The time of integration
15 microseconds；Integral number of times 20 times；Wavelength 200-400nm.
1.2.3 the foundation of Fundamental database is modeled
To testing sample S1-S6With paeonol reference substance sample B3, it is combined with spectrogrph by liquid chromatograph,
Gather this multi-wavelength light modal data after chromatographic column is kept completely separate of various kinds.From testing sample spectroscopic data
The spectroscopic data of middle deduction component to be measured paeonol, and through Data Dimensionality Reduction, obtain background spectra database N.
Liquid phase chromatogram condition: C18Post (4.6mm × 150mm)；Gradient elution, flow phase: 0～30min,
Acetonitrile: water=40:60 (V/V)；30～55min, acetonitrile: water=5:95 (V/V)；55～80min,
Acetonitrile: water=95:5 (V/V).Flow velocity 1mL/min；Sample size 20 μ L；Column temperature 20 DEG C；Chromatograph is examined
Survey wavelength 270nm.
Spectral conditions: floating cuvette (1cm)；The time of integration: 15 microseconds；Integral number of times: 20 times；
Ultraviolet detection wavelength: 200-400nm.
1.2.4 content detection of paeonol in sample to be tested
Above-mentioned standard spectral data storehouse V, background spectra database N and D are imported and calculate platform,
Choosing 200-400nm wavelength period, application vector-subspace angle criterion algorithm (being called for short VS method) is respectively
Calculate the content of paeonol in each sample to be tested.Wherein, in sample to be tested content detection of paeonol particularly as follows:
Step 4.1, set according to quantitative accuracy and reduce step delta (the present embodiment as 1000)；
Step 4.2, at formula yi=aix+biIn bring bigger x into1Value, obtains v1；
Described yiRepresent the absorbance of paeonol, a under i wavelengthi、biBeing constant, x represents Cortex Moutan
The concentration of phenol, v1Represent in concentration to be x1Time paeonol multi-wavelength absorbance y1, v1For all of
yiThe matrix of value composition；
Step 4.3, from sample to be tested spectroscopic data a deduct v1(the present embodiment is deduction Δ to/Δ
v1=v1/ 1000), the variable after deduction is designated as da；After background spectra database N and variable da is merged
It is designated as contrasting space M, calculates contrast space M and v1Angle；
Step 4.4, from sample to be tested spectroscopic data a, progressively deduct v1After, repeat step 4.3；
Step 4.5, after the paeonol in sample to be tested is deducted completely, comparison space M and paeonol
Spectral vector v1Space angle value there will be maximum θmax, record space angle maximum θmax
Corresponding during appearance reduce step number λ, by concentration x of paeonol1Estimate in sample to be tested with reducing step number
The content Y of paeonol1, calculating formula is Y1=X1× λ/Δ, the Y obtained1It is Cortex Moutan in sample to be tested
The content value of phenol.
2.3 response rate and Precision Experiment
Take 10ml S respectively2、S4And S5Each three parts, it is separately added into 8mg/L, 12mg/L, 16mg/L
Paeonol reference substance solution 10mL of three concentration, gathers its multi-wavelength ultraviolet mixed light after mix homogeneously
Spectrum.Use space angle criterion to calculate content value, calculate the response rate and the precision of the method.
3. result and discussion
The foundation in 3.1 paeonol standard spectrum storehouses
Preparation series concentration is the paeonol standard solution of 0.2～20mg/L, with 75% ethanol as blank,
Gather the 190nm-1100nm wave-length coverage spectrum of serial solution.Select 200nm-400nm wave-length coverage
Spectrum, obtains paeonol standard spectrum y after multivariate least square regressioni=aix+bi, it is designated as V,
Wherein linear equation, correlation coefficient at 270nm are: y=0.0792x-0.0636；R=0.9992.
The foundation of 3.2 Fundamental database
To paeonol reference substance solution B3With mixing sample S6Liquid chromatogram be analyzed.Such as Fig. 1
Shown in, A is the appearance time of paeonol, corresponds to 16.3～17.5min.From S6Spectroscopic data in
Deduction and paeonol have the spectroscopic data (such as A peak data in Fig. 1) of identical retention time, its remainder
According to (B peak data) then as the background data measuring paeonol content.Successively from sample S1-S5Light
It is stored in background after modal data is deducted the row corresponding to spectroscopic data of 16.3～17.5min time periods respectively
In data base, it is designated as M1～M5.Merge M1～M6Data constitute data base M.
The initial background spectroscopic data M data amount that liquid phase-spectrum combination obtains is big, if directly using, and fortune
Evaluation time is long, have impact on the ageing of method, it is therefore desirable to the data obtained are carried out dimensionality reduction to remove divisor
Noise according to and the dimension of redundancy, retain effect property data and can improve the processing speed of algorithm.Choosing
Judge that the main composition of system is 8 by the method for principal component analysis, by M through singular value decomposition, take U after degraded
Front 8 row of matrix, are the local data base N after dimensionality reduction, particularly as follows: application [U, S, V]=svd
(W) background spectra database W is carried out singular value decomposition dimensionality reduction, obtain m rank row after decomposition orthogonal
Matrix U, n rank row orthogonal matrix V and singular value matrix S, take the front q row of U, for the basis after dimensionality reduction
End data base N.
The mensuration of paeonol in 3.3 samples
Algorithm steps meter to the ultraviolet mixed spectra data spatially angle criterion of specimen sample S1～S5
Calculate the content of paeonol.The paeonol content value simultaneously calculated with high performance liquid chromatography is compared.Logical
Crossing calculating, content and the error analysis of the paeonol in different samples to be tested are as shown in table 1.
1 two kinds of distinct methods measurement results of table
Use space angle criterion result of calculation as can be seen from Table 1 and use high performance liquid chromatography to calculate knot
Fruit is close.Relative error is less than 1.80%, and the accuracy of method is preferable.
The 3.4 method response rate
The response rate the results are shown in Table 2.Sample recovery rate scope is at 97.33%-102.5% as seen from Table 2,
Relative error is less than 5.00%, and RSD value is 1.5218% (n=9).From the results, it was seen that with to
The content of the paeonol that amount-subspace angle criterion is calculated is close with actual addition, shows
The accuracy of the method is preferable.
Table 2 response rate is tested
3 conclusions
Herein by liquid phase-ultraviolet-visual spectrometer combination, apply subspace-angle criterion, establish pellet
Skin phenol content rapid analysis method.For the mensuration of similar sample, and only need to once model just can batch
Detection.Compared with high performance liquid chromatography, the method set up is reliable and stable, easy and simple to handle, and sample is not
Need complicated pre-treatment, quickly measure for paeonol content and provide a kind of practical quantitative analysis
Technology, and other paeonol goods detection field can be applied to.
Claims (5)
1., based on chromatograph-spectrogrph combination and an analysis method for the paeonol content of subspace angle criterion, its feature exists
In, specifically implement according to following steps:
Step 1, paeonol standard spectrum storehouse are set up,
Step 2, the preparation of sample to be tested and ultraviolet spectra collection,
Step 3, the foundation of modeling Fundamental database,
Content detection of paeonol in step 4, sample to be tested；
Content detection of paeonol in described sample to be tested is particularly as follows: by above-mentioned standard spectral data storehouse V, background spectra database N
And D imports and calculates platform, choosing 200-400nm wavelength period, application vector-subspace angle criterion algorithm calculates respectively respectively
The content of paeonol in sample to be tested；
The concretely comprising the following steps of content detection of paeonol in described sample to be tested:
Step 4.1, foundation quantitative accuracy set and reduce step delta；
Step 4.2, at formula yi=aix+biIn bring bigger x into1Value, obtains v1；
Described yiRepresent the absorbance of paeonol, a under i wavelengthi、biBeing constant, x represents the concentration of paeonol, v1Table
Show that in concentration be x1Time paeonol multi-wavelength absorbance y1, v1For all of yiThe matrix of value composition；
Step 4.3, from sample to be tested spectroscopic data a deduct v1/ Δ, the variable after deduction is designated as da；Bias light modal data
Storehouse N and variable da merges postscript and contrasts space M and v for contrast space M, calculating1Angle；
Step 4.4, from sample to be tested spectroscopic data a, progressively deduct v1After, repeat step (3)；
Step 4.5, after the paeonol in sample to be tested is deducted completely, the spectral vector v of comparison space M and paeonol1
Space angle value there will be maximum θmax, record space angle maximum θmaxCorresponding during appearance reduce step number λ, pass through
Concentration x of paeonol1The content Y of paeonol in sample to be tested is estimated with reducing step number1, calculating formula is Y1=X1× λ/Δ, obtains
Y1It is the content value of paeonol in sample to be tested.
Analysis based on chromatograph-spectrogrph combination with the paeonol content of subspace angle criterion the most according to claim 1
Method, it is characterised in that described paeonol standard spectrum storehouse is set up particularly as follows: prepare the pellet that series concentration is 0.2～20mg/L
Skin phenol standard solution, with 75% ethanol as blank, gathers the 190nm-1100nm wave-length coverage spectrum of serial solution；Select
200nm-400nm wave-length coverage spectrum, obtains paeonol standard spectrum y after multivariate least square regressioni=aix+bi, note
For V.
Analysis based on chromatograph-spectrogrph combination with the paeonol content of subspace angle criterion the most according to claim 1
Method, it is characterised in that preparation and the ultraviolet spectra collection of described sample to be tested are particularly as follows: take paeonol crystalline mother solution, room temperature
Under, take 0.15g upper solution and each portion of underlying crystalline respectively, be 10-20mg/L with 75% ethanol dilution to concentration, obtain
Sample S1And S2；
Take the paeonol crystalline mother solution two parts of different production batch, be separately heated to 50 DEG C and become molten condition, weigh 1.2g respectively
And 0.9g, it is 10-20mg/L with 75% ethanol dilution to concentration, obtains sample S3And S4；
Weigh paeonol crystalline product 0.1g, be 10-20mg/L with 75% ethanol dilution to concentration, obtain sample S5；Take S1-S5
Equal-volume is mixed to get sample S6；
Gather S1-S6Ultraviolet spectrum data, obtain sample to be tested data base, be designated as D；The time of integration 15 microsecond, integration time
Several 20 times, wavelength 200-400nm.
Analysis based on chromatograph-spectrogrph combination with the paeonol content of subspace angle criterion the most according to claim 1
Method, it is characterised in that described step 3 models the foundation of Fundamental database particularly as follows: to testing sample S1-S6And paeonol
Reference substance sample B3, it is combined with spectrogrph by liquid chromatograph, gathers this multi-wavelength after chromatographic column is kept completely separate of various kinds
Spectroscopic data；From testing sample spectroscopic data, deduct the spectroscopic data of component paeonol to be measured, and through Data Dimensionality Reduction, obtain this
End spectra database N；
Liquid phase chromatogram condition: 4.6mm × 150mm C18Post；Gradient elution, flow phase: 0～30min, acetonitrile: water=40:
60V/V；30～55min, acetonitrile: water=5:95V/V；55～80min, acetonitrile: water=95:5V/V；Flow velocity 1mL/min；
Sample size 20 μ L；Column temperature 20 DEG C；Chromatograph detection wavelength 270nm；Spectral conditions: floating cuvette 1cm；The time of integration:
15 microseconds；Integral number of times: 20 times；Ultraviolet detection wavelength: 200-400nm.
Analysis based on chromatograph-spectrogrph combination with the paeonol content of subspace angle criterion the most according to claim 4
Method, it is characterised in that in the dimensionality reduction of described background spectra database, it is suitable that described background spectra database W is reduced to
The method of dimension is as follows: application [U, S, V]=svd (W) carries out singular value decomposition dimensionality reduction to background spectra database W, decomposes
After obtain matrix with orthogonal rows U, n rank, m rank row orthogonal matrix V and singular value matrix S, take U front q row, after dimensionality reduction
Fundamental database N.
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| CN110208441A (en) * | 2019-01-17 | 2019-09-06 | 广西科技大学 | The rapidly extracting and detection method of concealed malachite green in fresh-water fishes |
| CN109765087B (en) * | 2019-01-17 | 2021-12-28 | 广西科技大学 | Method for rapidly extracting and detecting malachite green in freshwater fish |
| CN112086137B (en) * | 2020-08-18 | 2022-06-10 | 山东金璋隆祥智能科技有限责任公司 | Method for quantitatively analyzing sorbose content in fermentation liquor |
| CN111879717A (en) * | 2020-09-01 | 2020-11-03 | 江西纳弗堂制药有限公司 | Method for rapidly evaluating internal components and quality of traditional Chinese medicine formula granules |
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